Titania, titanium oxide (IV) or titanium dioxide is a semiconductor chemical compound having the formula TiO2. Among other applications, TiO2 is used in heterogeneous catalysis processes as support and/or catalyst.
Titanium oxide (IV) TiO2 is found in nature under various forms:                rutile (tetragonal structure),        anatase (tetragonal structure), and        brookite (orthorhombic structure).        
As nanostructures:                nanotubes,        nanosheets,        nanofibers, and        nanowires.        
Alumina or aluminum oxide is a chemical compound having the formula is Al2O3. Among other applications, it is used in heterogeneous catalysis processes as support and/or catalyst.
Aluminum oxide Al2O3 is found in nature under various forms:                Alfa-alumina (α-Al2O3 H2O corundum).        Beta-alumina (β-Na2.O12Al2O3).        Gamma-alumina (γ-Al2O3).        
Aluminum oxide Al2O3 is found in nature in the alumina octahedral structure in which 6 hydroxyl (OH—) groups or oxygen atoms are arranged in such a way that they form a vertex of an octahedron that is kept as a unit by an aluminum atom at the center.
As a semiconductor material, TiO2 features many advantages such as a wide band gap energy interval (Eg), high oxidizing power, biologically and chemically inert characteristics and no toxicity.
The catalytic features of TiO2 depend to a large extent on its chemical and physical properties, which are the ones that define its textural and morphological characteristics, specially its dimension and crystalline phase.
Specifically, the dimension of titania plays a major role in its catalytic properties, for example, nanostructured titania or TiO2 nanocrystals are currently a reference point regarding their applications, catalysis being one of the main fields.
The properties inherent to nanostructured titania or with nanometric crystal size are related to the crystal size diminution and the surface area increase with the corresponding dimension regarding the diameter and pore volume distributions. Nowadays, the nanostructured materials in their different versions (nanocrystals, nanotubes, nanofibers, nanospheres, nanosheets and nanowires) represent new alternatives and opportunities in their applications as materials that feature promising efficiency in a variety of fields.
These nanostructured materials show exceptional properties that are based on their special physicochemical features that grant them outstanding catalytic, magnetic, mechanical and optical characteristics.
Titania nanotubes were discovered in the 1990s; up to now, their main applications have been in photocatalysis and solar cells to produce energy. In these research works, it was found that titania nanotubes had both higher surface areas and interfacial charge transfer rates in comparison with TiO2 nanocrystals. For example, it was found that the positive charge transfer throughout the nanotubes can reduce the recombination of the electron-hole pair (Eg), which enables them to be highly efficient in photocatalytic decomposition reactions and photocells in comparison with TiO2 nanoparticles.
The synthesis of titania with specific characteristics regarding its structure (particles, fibers, sheets, wires, tubes, etc.) and size (nano), in addition to the understanding of its formation mechanism, are two of the most important points in the titania cutting-edge technology. Currently, new synthesis routes are being proposed to obtain TiO2 nanowires, nanotubes and nanofibers through electrochemistry, microwaves and condensed chemistry, which are still at research levels.
During the last decade, the methods that have been used for the synthesis of titania nanotubes are chemical vapor deposition (CVD), anodic oxidation and wet chemistry (sol-gel method and hydrothermal). The main aim of all these methods is to obtain special nanotube arrangements with better characteristics regarding the surface area and pore volume, and with specific structural arrangements. As for the condensed chemistry methods used to prepare titania nanotubes, the most recent are via surfactants, synthesis via alumina as template, via microwave irradiation, electrochemical synthesis and new routes of the hydrothermal method.
All the methods mentioned above have advantages and disadvantages regarding the final characteristics of the obtained titania nanotubes, for example, in the synthesis via alumina used as a template, it is possible to obtain uniform and well-aligned nanotubes, however, they are obtained with a higher dimension regarding their size due to the porosity of the alumina that serves as a mold, which yields pore diameters of up to 50 nm and, in general, their walls consist of TiO2 nanoparticles, which when trying to separate them, sometimes, some of them are destroyed, which makes this method not a really cost-competitive one.
As for the surfactant-based method, it is possible to obtain titania nanotubes with small pore diameters and very thin walls; in comparison with the other methods, its limitations are supported on long and complicated preparation processes, which increases their production costs.
By means of the hydrothermal method, titania nanotubes with sizes within the order of 10 nm are produced starting from titania nanocrystals, but by using a high concentration of sodium hydroxide, where the alkali ions are exchanged by protons to form H-titanates; with this method, different phases such as anatase, rutile and brookite are obtained, which depend on the synthesis temperature. As for this method, the mechanisms and the control of the formation ratio of the crystalline phases mentioned above are still under study, which seem to depend largely on the thermal treatments.
Preliminary studies on the formation of titania nanotubes starting from titania nanocrystals via hydrothermal methods have allowed the synthesis of nanotubes with diameters within the order of 8-10 nm, lengths within the order of 50-200 nm and specific areas within the order of 380-400 m2/g, where the Ti—O—Ti bonds are changed to Ti—O—Na; in this condition, the anatase phase exists under a metastable condition as “mild chemical reaction” at low temperature. As a next step in this method, HCl washings are carried out to perform the ionic exchange of Na by H and form once again the Ti—O—Ti bond, washing with deionized water to form either the Ti—OH or Ti—O°°°°H—O—Ti species. These materials have very specific applications, for example, in photocatalysis.
Some research lines point out that the hydrothermal treatment is a fundamental step to obtain titania nanotubes with special textural and morphological characteristics, placing the washing in second place, however, other lines establish the opposite, which means that they set the washing as a fundamental step in the synthesis of nanotubes. Other groups state that in each case, nanotubes for different applications are obtained.
Among the main debates regarding the use of either synthesis method, the types of nanotube crystalline structures that can be obtained is one of them, which can be the following: i) anatase/rutile/brookite TiO2, ii) lepidocrocite HxTi2-x[ ]x/4O4 (x˜0.7, [ ]: vacancies), iii) H2Ti3O7/Na2Ti3O7/NaxH2-xTi3O7, and iv) H2Ti4O9. Likewise, it is established that starting from the anatase phase, the nanotubes are easily formed in comparison with the method starting from rutile; another important factor is the crystal size from which one starts.
According to some studies, it was concluded that starting from titania powders in the anatase phase, nanotubes are easily obtained with improved order and structure size with respect to the route starting from rutile, where in addition, when these nanotubes are hydrated, they are transformed into hydrated hydrogen titanates (H2Ti3O7.nH2O(n>3)), obtaining a special morphology such as multiwall with a spacing within the order of 0.75-0.78 nm.
Some studies propose that the synthesis of tri-titanate nanotubes via hydrotreating can be achieved through two possible mechanisms: i) starting from titanium dioxide and a concentrated solution of sodium hydroxide (NaOH), obtaining Na2Ti3O7 as intermediary, being transformed into tri-titanates in the form of nanosheets (Ti3O7)2−), where this result depends on the NaOH concentration, to finally obtain titania nanotubes, however, not all H2Ti3O7 is transformed into titania nanotubes; ii) starting from sodium lepidocrocite Na2Ti3O7, which tends to form titania nanocrystals, but not stable, where the concentration of the Na+ ions also exerts an effect, to form nanocrystals and finally titania nanotubes.
It has been said that the expansion of titania particles promotes the formation of Na2Ti2O4(OH)2, where depending on the concentration of the NaOH solution, the short Ti—O bonds slide and expand to form lineal unions (unidimensional), O−—Na+—O−, to produce bidimensional flat fragments, where already as nanotubes, covalent bonds would be finally established.
An important factor in the application of the hydrothermal treatment is related to temperature, where it has been established that when titania reacts at high temperature (250° C.) in the presence of a NaOH solution, Na2Ti2O5°H2O is formed, where in order to remove the Na+ ions, it is washed with HCl in order to start the formation of sheets and after of nanosheets.
More specifically, the main factors that exert an effect on the formation of titania nanotubes with special physicochemical characteristics are those that are mentioned as follows, according to their sequence order in the hydrothermal method:                Synthesis precursors                    Rutile            Anatase            Degussa P25 nanoparticles            TiIV alkoxide            SiO2—TiO2 mixtures                        
In the synthesis of titania nanotubes via the hydrothermal method, the starting reagents play a major role, for example, starting from regular powders of an anatase/rutile mixture or from anatase/rutile nanocrystals or from titanate sheets (Na2Ti3O7) or from titanium salts (TiCl4) or from titania alkoxide (TiIV) or from doped TiO2 anatase or SiO2—TiO2 mixtures. In general, titania nanotubes with external diameters in the order of 10-20 nm can be synthesized starting from titania powders with big particle sizes such as TiO2-rutile, TiO2 Degussa (P25) or SiO2—TiO2 mixtures.
Taking as a reference the crystal sizes of starting materials, it was found that starting from TiO2 rutile with average particle sizes from 120 to 200 nm and with high concentration of NaOH (10 N) and at 150° C. for 48 h, nanotubes of the multilayer and “open-ended” (open) types with internal diameters and lengths around 2-3 nm and 50-200 nm, respectively, are obtained, in addition to a uniform rolling.
In addition, commercial titanias such as TiO2 Hombikat UV100 and TiO2 BCC100 have been used to obtain nanotubes with internal and external diameters of 3-6 nm and 7-10 nm, respectively, and with a length around 400 nm.
In recent studies, other types of materials have been used: i) fresh gels, ii) P-25 powders, and iii) TiO2 treated at 500° C. All these materials were submitted to the hydrothermal method. By using fresh gels, nanotubes with lengths in the order of 50-70 nm and with average diameter of 10 nm were obtained. With P-25 powders, the nanotubes showed diameters in the order of 50-300 nm. And with TiO2, nanotubes with several hundreds of nanometers and with an average diameter of 15 nm were obtained.                Hydrothermal method                    Ratio of NaOH Normality/Starting material (TiO2)            Operation conditions (time, stirring)            Synthesis temperature                        
In the hydrothermal method, the temperature plays a major role, for example, it is possible to form titania nanotubes with a temperature interval from 100 to 180° C. starting form TiO2 powders which can be a mixture of the anatase/rutile phases with yields from 80 to 90%; out the previous temperature interval, the formation of nanotubes decays. There is also a combination of a temperature interval with the NaOH concentration and the initial titania particle size, for example, at temperatures from 100 to 200° C. and 10 N NaOH and starting from TiO2 nanoparticles, the specific area and the pore volume of the obtained nanotubes are increased.
Another combination of variables regarding the hydrothermal method is the combination of the temperature and the aging time, for example, when an aging period of 72 h at 150° C. is carried out, a higher nanotube yield is obtained in addition to a defined crystallinity degree (titanates).
Most research works have stated that through the hydrothermal method, at temperatures below 100° C., nanotubes are not formed, obtaining nanosheets instead; likewise, it has been said that a vital step to form nanotubes is to start from sodium titanates, which appear at 70° C. as nanosheets and are transformed into nanofibers by increasing the temperature at 90° C.
By means of the hydrothermal method and at 160° C., the specific area and the pore volume in the nanotubes decrease due to the limitation of interlayer spaces and to the fact that the sodium ions are not replaced by hydrogen during the washing process with hydrochloric acid. In addition, at 170° C., nanorods appear with a diminution of the area and pore volume.                Pretreatments-Sonication                    Dispersion of nanoparticles            Inhibition of the crystal growth            Homogeneity of particles            Effect on the length distribution            Synergy in reactions                        
The sonication treatment of nanostructures is commonly used in nanotechnology to disperse nanoparticles, especially in liquid medium. As for the titania nanotubes, by means of this treatment in the hydrothermal method, the length can be controlled, and from the sonication rate depends the dispersion of nanoparticles for the intermolecular reaction between the TiO2 particles and the NaOH solution, in addition to make the system more homogeneous.
By means of the sonication treatment, the migration of the OH− and Na+ ions can be carried out throughout the restricted holes among the used titania precursor particles, which helps not delay the formation of nanotubes. Other properties that are attributed to the sonication treatment are that the average length of the obtained nanotubes is 3 to 9 times higher than without using this treatment, and the specific area is also increased.
On the other hand, the irradiation at different magnitudes within the interval from 100 to 280 W and up to 380 W exerts an effect on the morphology of the nanotubes, for example, between 100 and 280 W, small diameters (1 to 14 nm) are obtained and at high magnitude (380 W) it is remarkably increased from 199 to 600 nm. Likewise, the sonication during the preparation of nanotubes helps avoid the growth of TiO2 crystals. Definitely, the sonication treatment helps obtain nanotubes with higher lengths, small diameters and high specific areas.                Thermal treatments                    Effect on the structure of phases            Microstructures of the titanate nanotubes            Transformation of phases            Titanate nanotubes with anatase phase                        
The thermal post-treatments used after applying the hydrothermal method exert an important effect on the final morphology of the nanotubes. With the annealing treatments, it is possible to modify the obtained nanostructure via the hydrotreatment, for example, by means of heat, it is possible to transform again the titanates in the TiO2 anatase phase. Nanotubes have been stabilized at temperatures up to 500° C. with radii in the order of 8-22 nm, starting from pure anatase.
The temperature plays a major role in the crystallinity degree of the titania nanotubes, for example, TiO2 powders annealed at 400° C. form thin-wall nanotubes, but their structure is similar to the one of the material that was not submitted to this annealing temperature, however, in the interval from 600 to 800° C., the structure of the nanotubes collapses.
The effect by increasing the annealing temperature on the crystallinity and structure of the nanotubes is evident, for example, the crystal size is increased from 5 to 10 nm, the average pore size from 18 to 33 nm, the pore volume from 0.99 to 0.35 cm3/g and the specific area is diminished from 370 to 210 m2/g with a temperature increase from 300 to 600° C.
In general, after the washing process and at annealing temperatures above 500° C., the structure of the nanotubes is lost, being transformed into TiO2 nanoparticles, but with a higher crystal size than the one shown when submitted to the hydrothermal treatment to be transformed into nanotubes, likewise, in nanocrystals submitted to temperatures above 600° C., the anatase phase disappears gradually to be transformed into rutile.                Washing processes                    Establish elemental composition            Alignment of the specific area of the nanotubes                        
Most of the performed studies establish that the morphology and dimensions of the nanotubes are defined by the hydrothermal method, more than by the washing processes. Nevertheless, other studies do attribute them important effects such as the nanostructures or final phases of the nanotubes, their specific area and higher purity. During the washing process with HCl, the exchange of Na+ ions by H+ augments the spaces and thus the area.
The effect of the HCl concentration is also analyzed. It has been said that an interval of optimal concentration is from 0.5 to 1.5 M, where below 0.5 M, the elimination of Na+ is not efficient and above 1.5 M, the nanotubes can be destroyed, forming “clots” with sizes above 100 nm. Notwithstanding, in a study carried out with 0.1 M HCl at 150° C., a high nanotube efficiency was obtained and the length was also diminished.
Other studies sustain that when the Na+ ions are eliminated, the nanotubes are destroyed or the pore volume and the specific area are substantially diminished. It has also been assumed that when low NaOH concentrations (from 0.01 to 0.001 M) are used, the length of the nanotubes is of hundreds of nm with average diameters from 10 to 30 nm, being of the “open” or multi-wall types. Also, the combination of the starting TiO2 materials and the HCl concentration exert an effect, for example, starting from rutile TiO2 with 0.1 M HCl, nanoribbons are firstly obtained, but not all these nanostructures are transformed into nanotubes. That is why the washing process at a higher HCl concentration is essential if the formation of nanotubes is to be increased.
The XRD technique can be applied to both the qualitative or quantitative analysis of TiO2 nanostructures, where by means of this technique, it is possible to identify the types of present nanostructures, their proportions and dimensions. The previous information can be obtained by means of fundamental tools such as the Bragg Law and the Formula of the Integrated Intensities. The information that can be obtained is the following:                Space group and geometry of the unit cell, which are obtained from the collection of Bragg angles (2θ); likewise, from this information, a qualitative identification of the crystalline phases can be carried out;        Measurement of the crystal size by establishing the widening of peaks, which also helps establish the crystal purity;        Atomic positions in the unit cell by measuring the integrated intensities of the peaks, which in turn allows the quantitative analysis of the phases present in the sample, and;        Texture analyses, measurement of residual tensions and phase diagrams.        
By means of Fourier transform infrared spectroscopy (FTIR), it is possible to identify functional groups in the TiO2 nanostructures as it is the case of the identification of OH groups in nanotubes, which defines their hydroxylation degree, which is an important characteristic of titania as a catalytic material.
Likewise, the acid surface of supports and catalysts can be established; for this purpose, there are different methods: firstly, the adsorption of NH3 on the catalyst surface and secondly, the adsorption of pyridine, which is widely used as a probe molecule for the identification of both Lewis and Brønsted sites; in fact, this molecule can interact through the electron pair possessed by nitrogen (N) with the different sites. In general, the band located at 1640 and 1540 cm−1 is associated with Brønsted sites whereas the region located at 1630, 1440 and 1445 cm−1 is attributed to the coordination of Lewis sites; the band located at 1490 cm−1 is associated with both Lewis and Brønsted sites. As for ammonia, the main bands are located at the interval of 1850-1680 cm−1, which are related to the vibrations of NH4 chemisorbed on Brønsted sites; the bands located at 1600 and 1217 cm−1 are related to the vibrations of the N—H bonds coordinated on Lewis acid sites. Although both techniques help establish the types of sites present in the catalyst, the ammonia spectra are not that clear, for other types of bands can be overlapped, which causes problems to quantify the true acid sites, which is the opposite with pyridine, for the technique is more accurate and allows the cleaning of the zone where the adsorbed pyridine sites appear in order to quantify clearly the sites present in the supports or catalysts.
The measurements of the band gap energies (Eg) of TiO2 are fundamental to know its activity in catalytic processes, and are obtained from UV-vis spectra in the 200-800 nm region. In this region, the fundamental transition from the valence band to the conduction band is found; in this case for nanostructures of the nanotube or H-titanate types.
By means of the Transmission Electron Microscopy (TEM), it is possible to establish the morphology (phases), and the dimensions of the TiO2 nanostructures. Likewise, by selecting a crystal from different micrograph zones, it is possible to obtain the individual diffraction pattern, in addition to their corresponding interplanar distances with the software Digital Micrographs, which are compared with JCPDS classified cards for TiO2 (JCPDS.—Joint Committee on Powder Diffraction Standards), establishing in this way the crystal structure in the corresponding direction (hkl).
The physicochemical properties of a material are defined by the type of interactions that exist among electrons, and among ions and electrons; by reducing the space where the electrons can move, it is possible that new effects will appear due to the space confinement; this action makes that the energy levels where the electrons can be located inside the particles be modified. Due to the aforesaid and the fact that the surface/volume ratio is remarkably increased, the nanotubes show new properties that appear neither in the material at high amounts (“bulk”) nor in the fundamental entities of which the solid consists of.
There are two types of nanotechnology for preparing nanostructured materials:                The “Top-Down” method, which refers to the design of nanomaterials with size reduction (from big to a smaller size) and it is based on the mechanisms to obtain structures on nanometric scale. This type of nanotechnology has been used in different fields, being the electronics field the one with more applications, however, recently other fields are being incorporated such as those of medicine and environmental protection, and;        The “Bottom-Up” method, which refers to self-assembly processes that occur literally from a small size to a bigger size and starts with a nanometric structure such as a molecule and through a montage process or self-assembly, a mechanism bigger than the first one is created. This approach is considered as the only and “true” nanotechnological approach, which allows matter to be controlled extremely precisely on the nanometric scale.        
Some of their properties are:                Increase in the surface area/volume ratio, which induces a huge increase in the interfacial area of the surface species;        Changes in the electronic structure of the species that are part of the nanostructure;        Changes in the arrangement (crystalline structure, walls and distances and internal and external diameters, etc.) of the species in the nanotubes and the presence of defects, and;        Confinement and size quantum effects (quantum-size-effect) due to the confinement of the charge carriers inside the nanotube.        
Among the main patent documents in the state of the art of the technique, which the inventors identify as the closest to the present invention, are the following:                WO 2006/019288 A1 “A selective adsorbent material and its synthesis procedure” Feb. 23, 2006 by José Antonio Toledo and Maria Antonia Cortés Jacome, relates to a selective adsorption process of nitrogen and sulfur compounds present in different oil hydrocarbon fractions. The solid material used as an adsorbent consists of a nanostructured material with morphology of nanofibers and/or nanotubes of an inorganic oxide of a metal from the Group IVB with a specific area between 100 and 600 m2/g, which can be or not promoted with a transition metal. The materials of this patent can also be used as adsorbent materials of other contaminants and diverse materials, which is characterized by the steps of:        1. Selective adsorption of nitrogen compounds and/or with light and intermediate sulfur oil fractions, putting in contact such loads with a TiO2-x nanostructured material.        2. The nanostructured TiO2-x material with nanotubular morphology, high oxygen deficiency, beta phase crystalline arrangements and/or JT orthorhombic and/or anatase with or without transition metals.        3. Procedure for the preparation of nanostructured TiO2-x with transition metals, characterized by a hydrogen titanate and/or a mixed titanate of hydrogen and sodium, submitted to an ionic exchange with Cu and Zn oxides.        4. An adsorbent material such as nanostructured TiO2-x with specific areas from 50 to 500 m2/g and a pore size distribution from 2 to 10 nm.        5. An adsorbent material such as nanostructured TiO2-x with orthorhombic structure whose unit cell is described by the space group 59 Pmmm and shows an X ray diffraction peak at around 10 degrees on the 2Θ scale in the plane (200) and structure layers from 1 to 50.        6. An adsorbent material such as nanostructured TiO2-x characterized by a composition between 0 and 20 wt. % of Zn, Cu, Ni, Co, Fe, Ag, Mn, Cr, V, Mo or W, preferably Cu or Zn.        Where:        As starting material, the TiO2 anatase phase and/or TiO2 rutile phase and/or amorphous titanium hydroxide and/or directly the mineral known as rutile are employed;        Hydrothermal treatment of the previous aqueous solutions with stirring between 100 and 250 rpm, and at temperatures between 50 and 300° C., and at autogenous pressures from 1 to 50 atm;        Ionic exchange treatments with diluted acid solutions between 0.1 and 1M, using organic or inorganic acids such as hydrochloric, sulfuric, nitric, hydrofluoric, boric or phosphoric or ammonium salts capable of exchanging sodium within a pH interval from 1 to 7;        The nanostructured TiO2-x material, classified according to its crystallographic structure, established by X-ray diffraction as rutile type TiO2 or anatase and/or mixtures of both materials and/or amorphous titania, which due to its physicochemical properties can be used in the selective adsorption of nitrogen and/or sulfur compounds of light and intermediate oil fractions.        WO 2007/141590 A1 “Deposits of nanostructured titanium oxide via sol-gel for their use in the controlled release of pharmaceutical drugs in the nervous control system and its synthesis method”, published on Dec. 13, 2007 by López-Goerne T. refers to deposits of nanostructured TiO2 via sol-gel, which is compatible with brain tissue. In the nanostructured TiO2 of this patent publication, the pore size distribution, crystal size and the proportions of the crystalline phases (anatase, brookite and rutile) can be totally controlled. These materials can be used to contain neurological drugs and can be directly inserted into the brain tissue in order to control the release time of the drugs, which can be periods from 6 months to 3 years.        WO 2007/027079 A1 “Procedure for the preparation of a catalytic composition to hydroprocess oil fractions”, published on Mar. 8, 2007 by Toledo J. refers to the preparation process of a catalytic composition that comprises at least a no-noble metal from the Group VII and at least a metal from the Group VIB of the periodic table. The catalytic composition that is also a subject matter of this patent publication shows high specific activity in hydrotreating reactions of light and intermediate fractions, preferably in hydrotreating reactions of hydrocarbon currents such as hydrodesulfurization (HDS), hydrodenitrogenation (HDN) and hydrodearomatization (HDA).        WO 2007/027079 A “Sulfided catalysts of Mo/alumina-titania modified with nickel and palladium for the hydrodesulfurization of 4,6-dimetildibenzotiphene”, published on May 15, 2012, Vargas E. refers to the addition of Pd (0.3-0.8 wt. %) and Ni (NiO=3.1 wt. %) to Mo (MoO3=10.0 wt. %) in sulfided catalysts of alumina-titania (MO/AT). The addition of Pd and Ni to MO/AT catalysts exerts a positive effect producing a sulfided catalyst approximately 8 times more active for the HDS of the 4,6-DMDBT molecule, favoring the hydrogenation (HYD), promoting the elimination of S through a partially hydrogenated compound 4,6-TH-DMDBT, producing 3,3-DM-CHB. There is also an effect between Pd and Ni on the MO/AT catalyst, which is higher when Pd is incorporated to the Ni—Mo/AT catalyst than when Pd is incorporated to the MO/AT catalyst.        WO 2005/105674 A1 “Nanostructured titanium oxide material and its synthesis procedure”, published on Nov. 10, 2005, Toledo A. refers to titanium oxide nanostructured materials (TiO2-x where 0=x=1), which have an orthorhombic crystalline structure not yet known and that is the basic building unit of nanofibers, nanowires, nanorods, nanoscrolls, and/or nanotubes, which are produced from an isostructural precursor consisting of hydrogen titanates and/or a mixed titanate of sodium and hydrogen, which correspond to hydrogenated, protonated, hydrated and/or alkaline phases of such structures, which are obtained from titanium compounds such as titanium oxide with crystalline anatase structure, amorphous titanium oxide, titanium oxide with crystalline oxide structure and/or directly from the rutile mineral Y7O ilmenite. Likewise, the invention is related to the synthesis procedure of these materials.        CA 1,156, 210 (A1) “Preparation process of catalysts or catalyst supports based on titanium oxide and their use in the Claus process for sulfur synthesis”, published on Nov. 1, 1983, Dupin et al. discloses an improved procedure for synthesizing catalysts or catalyst supports based on titanium oxide for the Claus process for sulfur synthesis, which is characterized by the following stages:        1) A mixture is prepared containing from 1 to 40 wt. % of water up to 15 wt. % of conformation additive from 45 to 99 wt. % of badly crystalized titanium oxide powder and/or amorphous, which presents a loss on ignition between 1 to 50 wt. %;        2) The integration of this mixture is carried out, and;        3) The mixture is dried and the obtained products are annealed at temperatures between 200 and 900° C.        U.S. Pat. No. 6,034,203 A “Catalysis with titanium oxides”, published on Mar. 7, 2000, Lusting et al. discloses a process that can be used in oligomerization, polymerization or depolymerization processes, for example, the polyester production. The process puts in contact a carbonyl compound in the presence of a composition with an alcohol. The catalyst has the formula MxTi(III)Ti(IV)yO(x+3+4y)/2, where M is an alkaline metal, Ti(III) is titanium in the oxidation state +3, T(IV) is titanium in the oxidation state +4, and x and y are numbers greater than or equal to zero, where if x is equal to zero, y is a number lower than ½.        